Wet method of extracting copper, zinc, &amp;c., from their ores.



PATENTED NOV. 20, 1906.

. D. LANCE. WET METHOD OF EXTRAGTING' COPPER, ZINC, 8w, FROM THEIR ORES.

APPLIUATION FILED A UG. 7, 1905.

2 SHEETS-SHEET 1 Nnmus rzuns. In:vv umov. msmmnn, n

PATENTED Nov; 20, 1906.

. D. LANCE. WET METHOD OF EXTRAGTING GOPPER,-ZING,'&0-, FROM THEIR ORES.

APPLIOATION FILED AUG. 7, 1905.

2 SHEETS-SHEET 2 tied. It has likewise been observed that the co alt, and tungsten in the form of hydrated UNITED. STATES OFFICE. l v .DENIS LANCE, or PARIS, FRANCE.

' WETfMETHOD or EXIRACT'ING COPPERQ'ZINC, 4a., mom THEIR oars.

' Specification of Letters Patent. A lidaiionfiltd Au ie macs.- Serial nit-273063.

Patented Nov. 20, 1906;

To all whom it may concern.-'

of the French Republic, and a resident of Paris, France, have invented certain new and.

useful improvements in methods of extractin copper, zinc, cadmium, silver, IIlGkBl:

oxids direct from their ores by wet process, of which the following is a specification.

Simple or complex silicates may be rendered manageable by am'moniacal solutions, aminic solutions or ammoniaco-aminic solutions, it they be previously decomposed by a owerful acid actingalone or assisted by eat. r

4 In treatingnickel ores containing silicic acid, and particularly those from New Caledonia, Silesia, and Russia it is advisable for the-l urpose of quickly affecting the ore and att e same time rendering the effect more complete, to add to the ore, a certain quantity of a chlorid by sulfuric acid, and for this purpose to em- ,ploy' in lace of pure acid strongly-nitrous 3 peroxid acid in t e state in which it leaves the Gay Lussac tower.

In consequence of the reaction oi. the nitrous sulfuric acid on the chlorids,nitrosyl cblorid NOCl, as likewise nitry- 1 'chlorid NO Cl is generated, and these chloro-nitrates act rapidly on the ore containing silicic acid, and, in combination with the metals contained in this ore, form chlorids, setting free nitrogen dioxid (or nitric oxid) NO and the of nitrogen NO contained in the nytrosyl ,chlorid and in the nitrylchlorid. Again, these metallic chlorids, being immediately decomposed by the nitrous sulfuric acid, the compounds N001 and NO Cl are continually regenerated and the action on the ore roceeds perfectly.

Tiieoperation being carried on in a closed vessel, it will be understood that very small quantities of chlorids and of nitrous products are suflicient for affecting very consid erable quantities of ore. Moreover, the compounds N001 and NO Cl being rather volatile and almost insoluble in. water at the 'tem erature .of ,the'reaction, they can be easi y collected when the apparatus is empdrated, and the salts which are formed not being verysoluble in water a pro'tective" which is easily decomposed coating is formed around each portion of ore and quickly restricts the action. It is accordingly necessary during this action to introduce quantities of waterproportional thereto, so that the density of the acid is kept between and Bau'm if a good yield be desired. This action is further pro- V moted if during its progress the pulverizing of theme be continued, as if this be done any protective layer of salts" which may form around portions of the ore is destroyed by the pulverizing operation. Moreover, it has een observed that the yield, other things being equal, is greatest if the acid employed be previously heated to a tem erature of 110 to 120. Finally, it should be mentioned that it is desirable in the last stages of the reaction to employ a solutionof a bisulfate instead of simple water forthe purposes of hydration.

The observations referred to have led to a particular process which will be described, as employed for example, in the treatment of a New Caledonian nickel ore containing silicic acid.

j In the accompanying diagram the whole of 1 the operations can be followed, Figure 1 representing the first part of the installation and Fig. 2 the second part. These two parts can be joined together at the places indicated by broken lines in the two figures.

1 is a pyrite or soda furnace of the feed device, 2 and provided at 3 with retorts for the manufacture of the nitric acid. These retorts are heated by the waste heat and supplied with nitrate by the feed device 4. The nitric-acid vapors and the sulfurousfed by means acid vapors, as well as the necessary oxygen for the manufacture of the sulfuric acid, en-

ter the first lead-chamber 6 through the pipe 5. They. there mix with the steam coming from the boiler 7 through the pipe 8. The chambers 9 and 10 are two ordinary leadchambers, where the reactions take place.

11 is a Gay cle Lussac tower. The acid manufactured in the chambers 10, 9, and 6 reaches the top of the Gay de Lussac tower through the pipe 12. The nitrous sulfuric acid passes out at the bottom of the tower through the pipe 13, while the'nitrogen and the oxy gen in excess escape through the pipe 14 into the chimney. The nitrous sulfuric acid passes through the pipe 13, not into a Glover tower, but into the apparatus for sulfating the ore, which takes theplace thereof. These IIO apparatuses consist of Alsing, cylinders 16 and 17-, each having a leaden casing, a porcelain lining, and containing lumps of silex and furnished with axial pipes. To these cylinders the feed device 19 conveys the ore, which pipes '22, running from. the mainpipe '23., the

bisulfatefor example, the bisulfate of soda proceeding from the manufacture of the nitric acidbeing added by means of the feed devices 24 and 19.

For the purpose of heating the collection of apparatus and the acid to the temperature most favorable for the reaction, hot air, com- {ing from the flue 27 of the boiler 7 is caused to circulate in the Alsing cylinders 16 17 by means of the pump and the-pipe 26. This air passes out through the pi 2e 28 and comes under the fire-bars of the sulfurous-acid furnace, so that if in its passage it has taken up any nitrous vapors these vapors are restored to what is circulating chambers.

When the operationof sulfating theore is finishedthat is, after the action has continued from one-half to five hours, according to the nature of the oresthe nitrated compounds and chloro-nitrated compounds are discharged through the .pipe 29 into the pipe 3 5 5, from which they pass into the lead-chain:

here 6 9 10. The nitryl chlorid and nitrosyl chlorid play the same part (in fact, a more active part) in the manufacture of sulfuric acid as is played by the nitrosyl sulfate with which this manufacture is usuall effected.

The Alsing cylinders, in whic the sulfating operation is effected, thus act in the same way as the Glover tower, which, moreover, they replace, the nitrous or chloro-nitrous products being recovered in the cylinders at the end of'the reaction and restored to the .leadchamber andthe sulfuric acid being dischargedin the form of sulfate of the dissolved metals.

With the exception of the losses in work ing inherent in the manufacture of sulfuric acld the nitrous and chloro-nitrous products are constantly regenerated. Instead of hot air coming from the flue 27 being caused to circulate in the Alsing cylinders the mixture of sulfurous acid, nitric acid, and air which enters the first lead-cham-v ber 6 may be introduced direct into, these apparatuses. These gases, the Glover tower being dispensed with, are, in fact, at-a high temperature, too great for allowing of their being utilized in the lead chambers without prevlous cooling, which woulilfrender it necessary tomake the pipe 5, leading from the fur-v 6 nace 1 to the lead-chamber 6, rather long'. By

generally in the lead- 41, through t e pump 42, and the 1pe.-43.

conveying these gases into the Alsin cylinders the. greater part of this waste eat is utilized. .On the other hand, they will issue charged with. nitrous and chloro-nitrous vapors which were previously conveyed through the pi e 29 into the conduit5 in orderto mix with t em. Moreover, as they take up steam coming from the acid in the Alsing cylinders it is necessary, as when a Glover tower is employed, to provide the lead-chamber with a smaller uantity thereof. Under these conditions t e collection-of Alsing cylinders, in which the ore is treated most exactly and completely, replaces the Glover tower, the pulverised ore and the lumps of silex replacing the brick filling and the acid passing out freed from nitrous and chloro nitrous products in the form of sulfate of the metals which had to be dissolved. Thus the coo.- nomical advantages of that tower are utilized alike in the sulfating of the ore and in the manufacture of nitrous and chloro-nitrous pipe 34,fl-ows alternatelyinto one or the other of the filter-presses 35. The nickeliferous solution flows into. the receptacles 36-, then through the pipe 37 into the stirring-tank 38. The cake residue is emptied into the stirring-tank 39, situated below the filter-presses 35 and after having been diluted with-water entering through 40, and resulting from the last washing, asses through the filter-presses The second: nickeliferous solution t us obtained is likewise conveyed to the tank 38 by meansof vessels 44 and pipes 45 and 37'. The cake, as previously, is emptied into the tank 46 and steeped in the ordinary water coming through 47. The diluted mass is taken up by the ump 48 and passes to the press-filters 50 t ough the plpe 49. The small quantities of nickeliferous solution coming from the filter-presses 50 are conveyed, as

. was previously seen, to the last tank 39 by means of the vessels 51and the pipe 40. The exhausted sterile'mass is thrown into the gutter 52 and discharged through the central drain 53. The nickeliferous solution concentrated in 38 has an addition made to it at first of can; bonate of lime (ordinary limestone pulverized dry or moist) contained in the hopper 54, fed by the device 55, so as to effect the saturation of the greater part of the dissolved salts. This saturation is completed by the addition of seam.

the mass is conveyed to the filter-presses 58 through'the medium of the pump 59 and the from the filterpresses 58, and which shou d not causeany pipe 60. The liquid comin reaction in the soluble sulfids, is discharged throughthe vessels 61 and. the i e 62 into the central drain 53. The nicke liiierous calcic recipitate is emptied into the hopper 63 of t e feed device 64 and conveyed above the (o lixivi'ating-cylinders 65 66 6,7 resembling chloridating-casks. These cylinders 65 66 67 be ing charged, an ammomacal solution of 22 Baum, coming from the tank 68, is. introduced into them b? means of the pump 69 x and the pipe 70. his solution may be introduced into. all the a paratuses at once; but it is better to charge om one to the other and produce a methodical circulation of the fluid,

so that the liquor having remained a certain time in 65 passes into 66, then into 67, and

into the following apparatus if there be such,

and passes out completely saturated with oxid of nickel. In this way the cake is completely exhaused with the minimum of ammonia, and it is then sufiicient if distillation be effected'on the minimum of liquid.

The lixiviation having been effected in one apparatus, this being ascertained by, taking samples, the ammonia containing the sterile calclc matter is recovered by heating the mass at 100, which can be effected by means of the steam-pipe 71-, after, however, the largest'possible quantity of liquid has been expelled through the filtering-section 72 by means of the compressed air enterin through 73. This expulsion may also be e 'ected by the steam.- The ammonia-gas coming from the lixiviating apparatus during this operatio'n passes through the pipe 74 to the pipe 75, which collects the gases from the distilling-column 76. The nickeli'ferous ammoniacal solutions reach this same column through the pipe 77; but instead of reaching it direct they pass into the closed temperature-changers 78 79 throu h the pipe 80 and finally reach the top of t e column through the pipe 81. They are thus gradually. heated. T 1e column is heated by a steam-jet coming through the pipe 82, which branches oil 71. The ammonia-gas coming from the column, as well as that passing through 74 from the liXiviating-cylinders or any other part, passes through the pipe 75 to the tem erat'urechanger 79. 1t circulates in the coi ipe 83 55 then flows through the pipe 84 to the ottom of the condenser. Into this condenser, at the top, ordinary water enters through 86 or residuary water resulting from a previous operation and enterin through-87. The regenerated ammoniaca solution flows through 88 into the tank 68. The cycle is thus completed. The precipitated oxid of' nickel passes out with the residuary hot water from the column 76 through the pipe 89 and by 65. means of the pump 90 and t e pipe 91 this the pi coll'ectionis conveyed to the filter presses 92,

which are provided with hermeticall -closed casin s. he oxid of nickel remains etween the ates, (or stages and the residuary water disc arged into the casing passes through the pipe 93 into the coil-pipe 94 from the temperature-chan er 78 and flows in a cold state through t e pipe 87 at the top of the condenser, so that if in consequence of imperfect distillation or bad filtration they retain any '75 oxidwof nickel or ammonia, or both at once, these products reenter the general circulation without any loss being possible. Theoxid of nickel'is washed, if necessary, with ordinary Water flowinglfrom 86 or with the steam coming from 71, t en emptied into .the hopper 94 of a feed device 95, which conveys it to ordinary reducing apparatus.

If the washing be effected with water, the washing-waters issuing from 93 are combined with the residuary waters. If the washing be effected by steam, the small quantities or ammonia-gas pass through the pipe 96 and e 74 and mom the gases lssuing from the co umn 7 6. T e losses of ammonia, as of nickel, may thus be considered as reduced to v the smallest quantity possible in working. This collection of reactions and of apparatus is employed in the same manner as when complex, sulfurous, antimonious, or arsenic antimonious ores are treated instead of ores containing silicic acid.

Having now fully described my said invention, what I claim, and desire to secure by Letters Patent, is I 1. The herein-described process of extracting and concentrating metals from ores consisting in decomposing ores with' co'njointly reacting nitro sulfuric acid, decomposable metallic chloride, nitro-chlorids, oxide of nir05 trogen fumes, oxid of sulfur fumes and water vapors, in efiecting hydration of the herefrom-resulting salts of the metals contained in said ores, in separating said hydrated material and saturating with calcareous reagents, i 10 in separating the metalliferous calcareous recipitate and lixiviating with ammonia s0- utions, in removing the calcareous precipitate, in. distilling the liXiviation fluid, and in separatin v the precipitated metallic oxide.

2. The erein-described process of extracting and concentrating metals from ores consisting in treatin ores with nitrosulfuric acid and decomposable metallic chlorids, in causing nitrosulfuric acid to react upon decom- 12o, posable metallic chlorids to form nitrochlorids, in causing the said nitrochlorids to react upon the metal contained in said ore to form the chlorid of such metal, in causing the previously-added nitrosulfuric acid to react 1 25.

upon the sald metal chlorid to form the sulfate of the metal contained in said ore.

3.- The herein-described process of extracting and concentrating metals from ores consisting in treating ores with nitrosulfuric acid 1 0 and decomposable metallic chlorids in closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable metallic chloride to form nitrochlorids, in causing the 5 said nitrochlorids to react'upon the metal contained, in said ore to form the chlorid of such metal, in causing the previously-added nitrosulfurio acid to react upon the'said 1 metal chloridto form the sulfate of,the metal to contained in said'orein heatin to 110 to ect distil tion of the 1120" centigrade to e aforementioned nitrochlorids and in injecting oxid of sulfur fumes and water-vapors to.

4 form new quantities of sulfuric acid. 4i Thchorein-desoribcd process of extractiilg and oimcontrating metals from ores consistingin treating ores with nitrosulfuric acid and decomposable mgtalho chlorids in closed reaction-chambers, in causing nitrosulfuric an acid; to react upon. deoom osable" metallic chloride to form nitrcchlori s, in causing the stild nitroehlorids to react upon the metal contained in. said ere te -form the chlorid of such metal, in causing the previously-added nitresulfune acid. to. react upon the said metal chlorid to form thesulfate of the metal conta d: in said ore in heating to 110? to.

120 ecntigrade to sheet distillation of the tafoynnentioned 'nitroehlorids, in injecting watervapors to tern; new (Quantities of sulfuric acid, 111 eaus- 114 a cent nous eonoint-reactionbetween nilrosulfurle acid, econ posable metallic hl ride, nitrochlorids, oxids= of nitrogen mcs, 'mddmtsulfur fumes, watenvapors, e. metal contained. in. the ore and the chlo- -rid of the said metal, in causingthe cyclic formation of nitrosulfuric acid, nitrochlorids and the metal lo id, and in causin, the fora metion v p rmanent ul at oftfe metal conta d the said ore,

1 5'. The in=descrlb d process of extract ing and concentrating metals from ores conis ng in treatin ores with nitrosulfuric acid 5, and decomposab emetallic chloride in. closed reactiofi-ohambers, in causing nitrosulfuric acid to react upon decomposable metallic chlorids to form-nitrochlorids, in causing the said nitrochlorids to react upon the metal 50' co ained i said ore to form the chlorid of such metal, inueauslng the prevlouslwadded' nitrosulfurlc acid to react upont'he said metal hlorid tofonn the sulfate of the metal contained in said ore, ii -heating to 110 to s'glgtcentigrade to effect distillation ofthe a orementioned nitrochlorids, .11 injecting oxid-of-sulfur fumes and waterwapors to the metal chlorid, in causing the formation of permanent sulfate of the metal contained in thesaid ore,'in partially hydrating at 40 to Baum density and in completing the hydration with a metallic bisulfate.

6. The herein-described process of extractingand concentrating metals from ores consistmg in treating ores with nitrosulfuric acid and decomposable metallic'chlorids in closed reaction-chambers, in causing nitrosulfuric acid-to react upon decomposable metallic chlorids to form 'nitrochlorids, in causingthe said nitrochlorids' to react upon the metal contained in said ore to form the chlorid of i such metal, in causing the previously-added nitrosulfuricacid to react upon the said metal chlorid-to form the sulfate of the metal con-' tained in said ore, in heating to- 110 to 120 centigrade to effect distillation'of the aforementioned'nitrochlorids, in injecting oxidof-sulfur fumes and water-vapors to form new quantities of sulfuric acid, in causing a continuous conjoint reaction between nitrosulfuric acid,decomposable'metallic chlorids,

nitrochlorids, oxids0f-nitr ogen fumes, oXid' of-sulfur fumes, water-yapors, the metal contained in the ore and thechl0rid-of the said metal, in causing the cyclic formation of nitrosulfurio acid, nitrochlorids and the metal chlorid, in causing the formation of permanent sulfate of the metal contained in the said ore, in partially hydrating at 40 to 50 Baum density and in completing the hydrationwith sodium-bisulfate solution. 7. The herein-described process of extracting and concentrating metals from ores con- IOO sisting in treating ores with nitrosulfuric acid and decomposable metallic chloridsin .closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable .metallic chlorids to form nitrochlorids, in

causing the said nitrochlorids to react upon the metal contained in said ore to form the chlorid of such metal, in causing the pre vicusly-added nitrosulfuric acid to react upon the said metal chlorid to form the sulfate of the metal contained in said ore, in heating to .1 10 to 120 centigrade to effect distillation of the aforementionednitrochlorids, in injecting oxid-of-sulfur fumes andwater-va pors to form new quantitiesof sulfurictacid,

1n causing a continuous conjoint reaction betWecn nitrosulfuricacid, decomposable 1netallic chlorids, nitrochlorids, oxids of nitrogen fumes, oXid-of-sulfur fumes, water-va-.

pors, the metal contained in' the ore and the chlorid of the said metal, in causing the cy---' form new quantities of sulfuric acid, in causinga contmuous'conjoint reaction between 60 nitrosulfuric acid, decomposable metallic chlorids, m'trochlorids, oxids of -'nitrogen fumes, oxid-of-sulfur fumes, water-vapors, the metal contained in the ore and the chlorid of said metal in causing the cyclic forma- ,-65 ion 'of'nitrosulfuric, acid, nitroc orids and and in saturating the remaining liquid with calcareous reagents.

8. The herein-described process of extracting and concentrating metals from ores conchloridsto form nitrochlorids, in causing the said nitrochlorids'to react upon the metal contained in said ore to form the chlorid of such metal, in causing the previously-added nitrosulfuric acid to react upon the said metal chlorid to form the sulfate of the metal contained in said ore, in heating to 110 to 120 Centigrade to effect distillation of 'the aforementioned nitrochlorids, in inj ecting oXidof-sulfur fumes and water-vapors I to form new quantities of sulfuric .acid, in causlng a continuous con o1nt reaction between nltrosulfuric acld, decomposable me- 'tallic chlorids, nitrochlorids, oxids-ofmitrogen fumes, oxid-of-sulfur fumes, water-vapors, the metal contained in the ore and the chlorid of the saidmetal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorids and the metal chlorid, in causing the formation of permanent sulfate of the metal contained in the said ore, inpartially hydrating at 40 to Baum density, in completing the hydration with a metallicbis'ulfate, in

removing the non-metalliferous residuum from the hydrated reaction mixture and in saturating the remaining liquid with calcium carbonate and lime. 1

9. The herein-described process of extracting and concentrating metals from'ores consisting in treating ores with nitrosulfuric acid and decomposable metallicchlorids in closed reaction-chambers, in causing nitrosulfuric acid'to react upon decomposable metallic chlorids to formnitrochlorids, in causing the said nitrochlorids to react upon themetal contained in said ore. to form the chlorid of such metal, in causing the previously-added nitrosulfuric acid to react upon the said. metal chlorid to form the sulfate of the metal contained in said ore, in heating to 110 to 120 Centigrade to effect distillation of the aforementioned nitrochlorids,- in injecting oxid-Of-sulfur fumes and water-vapors to form new quantities of sulfuric acid, in causing a continuous conjoint reaction-between nitrosulfuric acid, decomposable metallic chlorids, nitrochlorids, oxids of nitrogen fumes, oxid-of-sulfur fumes, water-vapors,

the metal contained in the ore and the chlorid of the said metal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorids and the metal chlorid, in causing the formation of permanent sulfateof the metal contained inthe said ore, in partially hydrating at 40 to 50 Baum density, in completing thehydration with a metallic bisulfate, in

removing the non-metalliferous residuum rating the remaining liquid withcalcareous reagents, in separating the metalliferous calcio precipitateand in lixiviating the same with ammonia solutions.

in said ore, in heating to 110 to 120 centi-- grade to effect distillation of the aforementioned nitrochlorids, in injecting oxid-of-sulfur fumes and water-vapors to formnew quantities of sulfuric acid, in causing a continuous conjoint reaction between nitrosulfuric acid, decomposable metallic chlorids, nitrochlorids, oXids-of-nitrogen fumes, oxidof-sulfur fumes, water-vapors, the metal contained in the ore and the chlorid of the said metal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorids and the metal chlorid, in causing the formation of permanent sulfate of the metal contained in the said ore, in partially hydrating at 409 to 50 Baumdensity, in completing the hydration with a metallic bisulfate, in removing the non-metalliferous residuum from the hydrated reaction mixture, in saturating the remaining 1i uid with calcareous reagents, in separating t e metalliferous calcic precipitate and in lixiviating the same With ammonia solution. i

.11. The herein-described process of extracting and concentrating metals from ores consisting in treating ores with nitrosulfuric acid and decomposable metallic chlorids in closed reaction-chambers, in causmgnitrosulfuric acid to react upon decomposable metallic chlorids to form nitrochlorids, in causing the said nitrochlorids to react upon the metal contained in said ore to form the chlorid of such metal, in causing the previously-added nitrosulfuric acid to react upon the said metal chlorid, to formthe sulfate of the metal contained in said ore, in heating. to 110 to 120centigrade to-efl'ec't distillation of the aforementioned nitrochlorids, in inj ecting oXid-of-sulfurfumes and water-vapors to form new quantities of sulfuric aci in causing a continuous conjoint reaction be- I from the hydrated reaction mixture, in satutween nitrosulfuric acid, decomposable metallic chlorids, nitrochlorids, oxids-of-nitrogen fumes, oXid-of-sulfur fumes, Water-vapors,

the metal contained in the ore and the chlorid of the said metal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorids and the metal chlorid, causingthe formachlorid of such metal, in causing the prevition of permanent sulfate of the metal contained in the saidore, in partially hydrating at 40 to Baumjdensity, in completing the hydration with a metallic bisulfate, in removing the non-metalliferous residuum from the hydrated reaction mixture, in saturating e remaining liquid with calcareous reagents, in separating the metalliferou's calcic precipitate, in lixiviating the same with ammonia solutions, in removing the calcareous sediment and in distilling the lixiviation viously-ladded nitrosulfuric acid to react upon the said metal chlorid to form thesulfluid until freed from hydrogen nitrid.

12. The hereimdescribed process of' extracting and concentrating metals from. ores consisting in treating ores with nitrosulfuric acid and decomposable metallic chlorids in closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable metallic chlorids to form nitrochlorids, inv

causing the said nitrochloridsto react upon the metal containedin said ore to form the chlorid of such metal, in causing the prefate of the metal contained'in said ore, in heating to 110 to 120 centigrade to effect distillation of the aforementioned nitrochlorids, in injecting oxid-of-sulfur fumes and water-vapors to form new quantities of sulfuric' acid, in causing a continuous conjoint reaction between nitrosulfuric acid, decomposable metallic chlorids,nitrochlorids, oxidsof-nitrogen fumes, oxid-of-sulfur fumes, water-vapors, the metal contained in the ore and the chlorid of the said metal, in causing the cyclic formation of nitrosulfuric acid,

- nitrochlorids and the metal chlorid, in causl'tallicoxid precipitated thereby.

13. The herein-described process of extracting and concentrating metals from ores consisting in treatin ores with nitrosulfuric acid and decomposale metallic chlorids in closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable metallic chlorids to form nitrochlorids, in causing the said nitrochlorids to react upon the metal contained in said ore to form the ously-added nitrosulfuric acid to react upon the said metal. chlorid to form the sulfate of the metal contained in said ore, in heating to 110 to 120 centigrade to effect distillation;

of the aforementioned nitrochlorids, in injecting oxid-of-sulfur fumes and Water-vapors to form new quantities of sulfuric acid, in causing a continuous conjoint reaction between nitrosulfuric acid, decomposable metallic chlorids, nitrochlorids, oXids-of-nitrogen fumes, oxid-of-sulfur fumes, water-Va ors, the metal contained in the ore and the ch orid of the said metal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorid's-and the metal chlorid, in causing the formation of permanent sulfate of the metal contained in the said ore, in recovering the aforesaid nitrochlorids by distillation and in using the same in subsequent decompositions of ores iniplace of new charges thereof. i

14. The herein-described process of extracting and concentrating metals from ores consisting in treating ores with nitrosulfuric acid and decomposable metallic chlorids in closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable me tallic chlorids to form nitroclrlor1ds,'in causing the said nitrochlorids to react upon the metal contained in said ore to form the chlorid of such metal, in causing the previously-added nitrosulfuric acid to react upon the said metal chlorid to form the .sulfate of the metal contained in saidore, in heating to 110 to 120 centigrade .to effect distillation of the aforementioned nitrochlorids, in injecting oXid-of-sulfur fumes and water-vapors to. form new quantities of sulfuric acid, in

causing a continuous conjoint reaction between nitrosulfuric acid, decomposable metallic chlorids nitrochlorids, oxi ds-of-nit-rogen fumes, oxid-of-sulfur fumes, water-vapors, the metal contained in the ore and the chlorid of the said metal, in causing the cyclic formation of nitrosulfuric acid, nitrochlorids and the metal chlorid, in causing the formation of permanent sulfate of the metal con tained in the said ore, in partially hydrating at 40 to 50 Baum density, in completing the hydration with a metallic bisulfate, in removing the non-metalliferous residuum from the hydrated reaction mixture, in saturating the remaining liquid with calcareous reagents, in separating the metalliferous calcic precipitate, in lixiviating the same with ammonia solutions, in removing the calcareous sediment, in recovering the residual ammonia from the said calcareous sediment and in using the recovered ammonia in subsequentlixiviations in place of new charges thereof. i

15.- The herein-described process of extracting and concentrating metals from ores consisting in treating ores with-nitrosulfuric acid and decomposable metallic chlorids in closed reaction-chambers, in causing nitrosulfuric acid to react upon decomposable me-,

tallic chlorids to form nitrochlorids, incausing the said nitrochlorids to react uponthe metal contained in said ore to form the chlorid of such metal, in causing the pre-- lic formation of nitro'sulfuric acid, nitrochlorids and the metal chlorid, in causing theformation of permanent sulfate of the metal contained in the said ore, in partially hydrating at 4:0 to 50? Baum density, in completing the hydration with a metallic bisulfate, in removing the non-metalliferous residuum from the hydrated reaction mixture, in saturating the remaining liquid with calcareous reagents in separating the metalliferous calcic precipitate, in lixiviating the same with ammonia solutions, in removing the calcareous sediment, in distilling the lixiviation fluid until freed from ammonia, in recovering the said distilled ammonia and in using the same in subsequent lixiviations in place of new charges thereof.

16. The herein-described rocess of extracting and concentrating nickelfrom silicious nickel ore, consisting in treating said ore with nitrosulfuric acid and sodium chlorid in closed reaction chambers, in cansing nitrosulfuric acid to react upon sodium chlorid to form nitrochlorids, in'causing the said nitrochlorids to react 11 on the nickel contained in said ore to form 0 lorid of nickel, in causing the previously-added nitrosulfuric acid to react upon the said nickel chlorid to form sulfate of the nickel contained in said ore, in heating to 110 to 120 centigrade to effect distillationof the aforementioned nitrochlorids, in injecting o'Xid-of-sulfur fumes and water-Va ore to form new quantities of-sulfuric aci in causing a continuous conjoint reaction between nitrosulfuric acid, sodium chlorid, nitrochlorids, oxids of nitrogen fumes, oX1dofsul fur fum es, Water-vapors, the nickel of said ore and chlorid of nickel, in causing the cyclic formation of nitrosulfuric acid,

nitro chloride and nickel chlorid, in causing formation of permanent sulfate of the nickel con-- tained in said ore, in partially hydrating at 40 to Baum density, in completing the hydration with sodium bisulfate solution, in removing the non-metalliferous residuum of the silicious ore from the hydrated reaction miX ture, in saturating the remaining liquid with metalliferous calcic precipitate, in lixiviating' the same with ammonia solutions in removing the calcareous sediment, in distilling the lixiviation solution until freed from ammonia and-in separating the hydrated nickel oxid precipitated thereby.

In testimony whereof I have hereunto set my hand in presence of two witnesses.

calcium carbonate andlir'ne,in separating the DENIS LANCE.

Witnesses: ADoLPHE STURM, HANSON C.COXE. I 

